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CN106591384A - Comprehensive treatment method of xylose mother liquor - Google Patents

Comprehensive treatment method of xylose mother liquor Download PDF

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Publication number
CN106591384A
CN106591384A CN201611194776.7A CN201611194776A CN106591384A CN 106591384 A CN106591384 A CN 106591384A CN 201611194776 A CN201611194776 A CN 201611194776A CN 106591384 A CN106591384 A CN 106591384A
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xylose
mother liquid
xylose mother
arabinose
mother liquor
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罗国伟
陈德水
徐小荣
廖承军
毛宝兴
江松涛
朱圣伟
周元
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Zhejiang Huakang Pharmaceutical Co Ltd
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Zhejiang Huakang Pharmaceutical Co Ltd
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    • C12P19/00Preparation of compounds containing saccharide radicals
    • C12P19/14Preparation of compounds containing saccharide radicals produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase, e.g. by cellulase, hemicellulase

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Abstract

The invention discloses a comprehensive treatment method of a xylose mother liquor. The method includes: (1) adding a flocculant into the xylose mother liquor, performing stirring and controlling the material temperature, carrying out filtering to obtain an impurity removed xylose mother liquor; (2) subjecting the impurity removed xylose mother liquor to enzymatic oxidation at 35-45DEG C by immobilized glucose oxidase resin to obtain gluconic acid-containing oxidation liquid, collecting the oxidation liquid and performing treatment to obtain sodium gluconate crystals; (3) carrying out xylose polymerization reaction on glucose removed xylose mother liquor through an immobilized xylanase bed so as to obtain a xylooligosaccharide-containing polymer liquid, collecting the polymer liquid and performing treatment to obtain xylooligosaccharide powder; and (4) conducting chromatographic separation on the xylose removed xylose mother liquor to obtain L-arabinose rich fraction, and treating the fraction so as to obtain L-arabinose crystals. The method provided by the invention separates and recovers components with high economic benefits in the xylose mother liquor one by one, realizes the effect of co-production of multiple effective components, and improves the comprehensive utilization efficiency of the xylose mother liquor.

Description

A kind of integrated conduct method of xylose mother liquid
Technical field
The present invention relates to the preparation technology of xylose or xylitol, more particularly to a kind of integrated conduct method of xylose mother liquid.
Background technology
Xylose is a kind of pentose.Natural D- xyloses are present in plant with the form of polysaccharide, wherein many in corn cob Contracting pentose content highest.Xylose can manufacture xylitol by hydrogenation.Xylitol is a kind of natural, healthy sweeting agent, sugariness Suitable with sucrose, xylitol is not cariogenic and has anticariogenic effect, and metabolism is not adjusted by insulin, complete in human body metabolism Entirely, can be used as the heat energy of diabetes patient.
At present the production method of xylitol is mainly chemical method, i.e., (contain 36 rich in poly-pentose using corn cob, bagasse etc. ~40% pentosan) raw material, Jing acid hydrolysis into containing xylose hydrolyzed solution, then neutralized, decolouring, ion exchange, knot The complicated purification process such as crystalline substance isolates and purifies out xylose from hydrolyzed solution, then makes xylose generate xylose xylose chemistry hydrogenation Alcohol.
It is above-mentioned prepare xylitol during can produce substantial amounts of xylose mother liquid, xylose mother liquid is stayed after xylose crystalline The deeper thick liquid of color, the total sugar content of the xylose mother liquid of different manufacturers and different lot numbers is different, it is general come Say, sugared concentration about 50~60% in xylose mother liquid, xylose, L-arabinose, glucose, galactose, mannose etc. are contained in the inside Various saccharic compositions, wherein glucose contain 12~18% or so, and xylose contains 40~50% or so, and arabinose contains 17~23%, half Lactose contains 0~6%.
Because the miscellaneous sugar content inside xylose mother liquid is higher, the dissolubility for causing xylose therein and L-arabinose increases Greatly, traditional method is caused to crystallize out.At present xylose mother liquid is also failed to be used well, typically gone out with low price Caramel color factory is sold to, the benefit of xylose alcohol production is greatly reduced, while causing the substantial amounts of wasting of resources and serious environment Pollution.
The content of the invention
The present invention provides a kind of integrated conduct method of xylose mother liquid, is individually separated extraction and obtains sodium gluconate, oligomeric Xylose and L-arabinose, are comprehensively utilized xylose mother liquid, improve the economic worth of xylose mother liquid.
A kind of integrated conduct method of xylose mother liquid, including:
(1) flocculant, stirring and control material temperature are added in xylose mother liquid, the xylose Jing after filtering and obtain remove impurity is female Liquid;
(2) xylose mother liquid after remove impurity is carried out into oxydasises at 35~45 DEG C by immobilized glucose oxidase resin, The oxidation solution containing gluconic acid is obtained, oxidation solution is collected and process is obtained gluconic acid sodium crystal;
(3) xylose mother liquid for removing glucose is carried out into xylose polyreaction by Immobilized Xylanase bed, is contained There is the polymer fluid of oligomeric xylose, collect polymer fluid and process obtains xylo-oligosaccharide powder;
(4) xylose mother liquid for removing xylose is carried out into chromatographic isolation, obtains the fraction rich in L-arabinose, the fraction L-arabinose crystal is obtained Jing after processing.
The mass percent concentration of total sugar is 45~60% in heretofore described xylose mother liquid, and wherein xylose accounts for total sugar 40~55%, L-arabinose accounts for the 15~25% of total sugar, and glucose accounts for the 10~25% of total sugar, and galactose accounts for the 5 of total sugar ~10%, and on a small quantity other sugared parts account for the 10~15% of total sugar.
In step (1), the impurity in xylose mother liquid is removed by flocculation, preferably, dry by sugar liquid in xylose mother liquid 0.3~1.0 addition flocculant of amount of substance degree, control material temperature is 50~80 DEG C, is stirred 20~50 minutes, is stirred Mix rotating speed is 100~500 revs/min.
Preferably, in step (2), it is 2~6 to control xylose mother liquid by the speed of immobilized glucose oxidase resin Times immobilized glucose oxidase resin volume/hour.Xylose mother liquid is at such speeds by immobilized glucose oxidase tree Fat, it is ensured that the glucose in xylose mother liquid is fully converted into gluconic acid.
Preferably, in step (2), the process of oxidation solution includes:
(2-a) oxidation solution is controlled into the electrical conductivity < 10us/cm of effluent by anion exchange resin;
(2-b) mass percent concentration is adopted to wash to anion exchange resin for 7~10% sodium hydroxide solution De-, eluent is sodium gluconate solution;Sodium hydroxide solution pump into anion exchange resin volume that speed is 3~4 times/ Hour;
(2-c) eluent decolourized, concentrated, being centrifuged, being dried, being obtained gluconic acid sodium crystal.
Preferably, in step (3), the pH value of xylose polyreaction is 5~6, and temperature is 45~65 DEG C, and control removes Portugal The xylose mother liquid of grape sugar is by Immobilized Xylanase bed volume that the speed of Immobilized Xylanase bed is 0.3~4.5 times/little When.
Under the reaction conditions, by controlling enzyme reaction balance, enzyme reaction is made to carry out to the direction for generating oligomeric xylose, will Xylose is the higher oligomeric xylose of economic worth, realizes the recycling to xylose in xylose mother liquid.
It is further preferred that the pH value of xylose polyreaction is 5~5.5, temperature is 50~60 DEG C, and control removes glucose Xylose mother liquid by Immobilized Xylanase bed volume/hour that the speed of Immobilized Xylanase bed is 0.3~1 times.
Under the reaction conditions, the conversion ratio of xylose is higher.
Preferably, in step (3), the process of polymer fluid includes:
By polymer fluid by the NF membrane that molecular cut off is 100~300KD, volume ratio is obtained for 1:3~5 raffinate With extracting solution, oligomeric xylose is rich in raffinate, concentrated, centrifugation, drying obtain xylo-oligosaccharide powder.
Jing after a membrance separation, oligomeric xylose is separated not thoroughly, more oligomeric xylose is also contained in extracting solution, further Preferably, secondary membrance separation is carried out to extracting solution and obtains secondary raffinate and secondary raffinate, raffinate will be merged twice.
It is further preferred that it is 90~95% to control oligomeric xylose content in the raffinate after merging, in secondary raffinate Oligomeric xylose content < 5%.
Also contain unpolymerized xylose in secondary raffinate, it is further preferred that by secondary raffinate and removing glucose Xylose mother liquid with volume ratio as 2~5:1 mixing, aggregated reaction and membrance separation, until xylose contains in the extracting solution of membrance separation Amount < 10%.
Jing after aforesaid operations, the xylose in xylose mother liquid can be fully converted into oligomeric xylose and be reclaimed, fully be gone back Receive the recycling that L-arabinose in xylose mother liquid is also beneficial to after the xylose in xylose mother liquid.
L-arabinose is combined in extracting solution in step (3), preferably, in step (4), with pure water as eluant, With chromatographic isolation resin as separating medium, the xylose mother liquid to removing glucose and xylose carries out chromatographic isolation, chromatographic isolation temperature For 45~60 DEG C, eluant flow velocity is 1.5~3.0m3/h。
It is further preferred that the process of the fraction rich in L-arabinose includes:
(4-a) fraction that will be enriched in L-arabinose is concentrated to dryness amount of substance percent concentration for after 50~70%, by sugar 0.1~0.5 addition activated carbon of liquid amount of dry matter degree, control material temperature is 50~80 DEG C, and speed of agitator is 60 ~150 revs/min, insulation is filtered after 20~50 minutes;
(4-b) by filtrate Jing ion exchange resin remove impurity, and be further concentrated to dryness amount of substance percent concentration for 65~ 75%, Jing cooling crystallization, centrifugation, drying, obtain L-arabinose crystal.
Compared with prior art, beneficial effects of the present invention are:
(1) present invention successfully one by one separates and recovers the composition of high financial profit in xylose mother liquid, obtains various high-purity Degree composition, realizes the effect of many effective ingredient coproduction, improves the comprehensive utilization ratio of xylose mother liquid, advantageously reduces production Cost;
(2) balance of flexible utilization enzymatic conversion reaction, by xylose the higher oligomeric xylose of economic worth is produced.
Description of the drawings
Fig. 1 is the schematic flow sheet of the integrated conduct method of xylose mother liquid in embodiment.
Specific embodiment
The mass percent concentration of total sugar is 45~60% in the xylose mother liquid of following examples, and wherein xylose accounts for total sugar 40~55%, L-arabinose accounts for the 15~25% of total sugar, and glucose accounts for the 10~25% of total sugar, galactose account for total sugar 5~ 10%, and on a small quantity other sugared parts account for the 10~15% of total sugar.The integrated conduct method of xylose mother liquid in following embodiment Flow process is as shown in Figure 1.
Embodiment 1
(1) remove impurity:By 0.3 addition flocculant of sugar liquid amount of dry matter degree, control material in xylose mother liquid Temperature is 50 DEG C, and speed of agitator is 100 revs/min, is incubated 20 minutes, is then filtered with flame filter press, obtains the wood after remove impurity Sugared mother solution;
(2) separating glucose acid sodium:
A, oxydasises:Xylose mother liquid after remove impurity is pumped in immobilized glucose oxidase resin column, 40 DEG C of temperature Under constant temperature, oxydasises are carried out, it is 3 times of immobilized glucose oxidase resin volume/hours that xylose mother liquid pumps into speed, until mistake Till flowing out without gluconic acid in the oxydasises liquid of post, oxydasises liquid is collected, carry out ion exchange;
B, anion exchange and regeneration:Oxydasises liquid pump is entered in anion exchange resin, anion exchange is carried out, is pumped into Speed is 6 times of anion exchange resin volume/hours, is monitored by on-line chromatograph work station, until without Fructus Vitis viniferae in effluent Till saccharic acid;In regenerative process, first pump into 3 times of resin anion (R.A.) volume purified water and washed, collect effluent and with before Effluent merges, and by pumping into 7% sodium hydroxide solution eluting is carried out, and the speed that pumps into of sodium hydroxide solution is 3 times of negative resins Volume/hour, without till sodium gluconate in eluent;Eluent is obtained through subsequent concentration, centrifugation, drying steps To gluconic acid sodium crystal, the purity of gluconic acid sodium crystal is 96.54%, and yield is 78%;
(3) separating oligomeric xylose:
A, enzymatic conversion are separated with oligomeric xylose:By the pH regulator for removing the xylose mother liquid after glucose to 5.5, fixation is pumped into In changing the fixed bed of xylanase, volume is pumped into for 0.5 times of fixed bed volume/hour, 55 DEG C of fixed bed jacket heat-preservation, from fixation Oligomeric xylose content is 10% in the enzymatic conversion liquid flowed out in bed, collects the effluent after enzymatic conversion, is directly entered NF membrane point From system, raffinate is 1 with extracting liquid volume ratio:5, secondary membrance separation is carried out to extracting solution, merge raffinate twice, finally carry Extraction raffinate oligomeric xylose content is 95.43%, and it is 40.86% that extracting solution oligomeric xylose content is 2.18%, Xylose Content, will be extracted Liquid is by volume 3 with xylose mother liquid after glucose is removed:1 mixing, then Jing enzymatic conversions, membrance separation, until the wood in extracting solution Sugared content < 10%;
B, extraction oligomeric xylose:Add by the 0.2 of raffinate amount of dry matter degree in nanofiltration membrane separation raffinate Plus activated carbon decolourized, ion exchange remove impurity, be finally concentrated to dryness amount of substance percent concentration to carry out spray dried after 50% Dry, inlet temperature is 180 DEG C, and leaving air temp is 85 DEG C, and charging rate is 1m3/ h, finally obtains xylo-oligosaccharide powder, oligomeric xylose The purity of powder is 94.32%, and yield is 93.77%;
(4) L-arabinose is separated:
A, L-arabinose are separated:Final extracting solution after by nanofiltration separation is pumped in chromatographic separation device, is with pure water Eluant, with chromatographic isolation resin as separating medium, to nanofiltration membrane separation after final extracting solution in component separate, separate Temperature is 55 DEG C, and separation flow velocity is 2.5m3/ h, extracting solution is separated into two fractions, and a part is based on L-arabinose The content of fraction, wherein L-arabinose is more than 70%;Another part is the fraction based on miscellaneous sugar, collects two kinds respectively and evaporates Point;
The extraction of b, L-arabinose:Take the fraction based on L-arabinose and measure amount of dry matter percent concentration and be 30%, the fraction is concentrated to dryness into amount of substance percent concentration for after 50~70%, by sugar liquid amount of dry matter degree 0.3 addition activated carbon, control material temperature is 60 DEG C, and speed of agitator is 100 revs/min, and insulation uses flame filter press after 30 minutes Filter, then Jing anion-cation exchange resins remove impurity, and it is 70% to be further concentrated to dryness amount of substance percent concentration, is imported normal Crystallization is cooled down in piezocrystallization tank, make L-arabinose crystal separate out, most after Jing centrifugation, drying process obtain L- I Primary sugar crystal, the purity of L-arabinose crystal is 99.36%, and yield is 90.44%.
Embodiment 2
(1) remove impurity:By 1.0% addition flocculant of sugar liquid amount of dry matter degree in xylose mother liquid, thing is controlled Material temperature degree is 80 DEG C, and speed of agitator is 500 revs/min, is incubated 50 minutes, is then filtered with flame filter press, after obtaining remove impurity Xylose mother liquid;
(2) separating glucose acid sodium:
A, oxydasises:Xylose mother liquid after remove impurity is pumped in immobilized glucose oxidase resin column, 35 DEG C of temperature Under constant temperature, oxydasises are carried out, it is 2 times of immobilized glucose oxidase resin volume/hours that xylose mother liquid pumps into speed, until mistake Till flowing out without gluconic acid in the oxydasises liquid of post, oxydasises liquid is collected, carry out ion exchange;
B, anion exchange and regeneration:Oxydasises liquid pump is entered in anion exchange resin, anion exchange is carried out, is pumped into Speed is 6 times of anion exchange resin volume/hours, is monitored by on-line chromatograph work station, until without Fructus Vitis viniferae in effluent Till saccharic acid;In regenerative process, first pump into 3 times of resin anion (R.A.) volume purified water and washed, collect effluent and with before Effluent merges, and by pumping into 10% sodium hydroxide solution eluting is carried out, and the speed that pumps into of sodium hydroxide solution is 4 times of negative resins Volume/hour, without till sodium gluconate in eluent;Eluent is obtained through subsequent concentration, centrifugation, drying steps Gluconic acid sodium crystal, the purity of gluconic acid sodium crystal is 95.87%, and yield is 79.17%;
(3) separating oligomeric xylose:
A, enzymatic conversion are separated with oligomeric xylose:By the pH regulator for removing the xylose mother liquid after glucose to 5, immobilization is pumped into In the fixed bed of xylanase, volume is pumped into for 0.3 times of fixed bed volume/hour, 45 DEG C of fixed bed jacket heat-preservation, from fixed bed Oligomeric xylose content is 8% in the enzymatic conversion liquid of middle outflow, collects the effluent after enzymatic conversion, is directly entered nanofiltration membrane separation system System, raffinate is 1 with extracting liquid volume ratio:5, secondary membrance separation is carried out to extracting solution, merge raffinate twice, last raffinate Oligomeric xylose content be 90.98%, extracting solution oligomeric xylose content be 2.25%, Xylose Content be 45.74%, by extracting solution with It is by volume 2 to remove xylose mother liquid after glucose:1 mixing, then Jing enzymatic conversions, membrance separation, until the xylose in extracting solution contains Amount < 10%;
B, extraction oligomeric xylose:Add by the 0.2 of raffinate amount of dry matter degree in nanofiltration membrane separation raffinate Plus activated carbon decolourized, ion exchange remove impurity, be finally concentrated to dryness after amount of substance percent concentration 50% and be spray-dried, Inlet temperature is 180 DEG C, and leaving air temp is 85 DEG C, and charging rate is 1m3/ h, finally obtains xylo-oligosaccharide powder, xylo-oligosaccharide powder Purity be 90.51%, yield is 90.66%;
(4) L-arabinose is separated:
A, L-arabinose are separated:Final extracting solution after by nanofiltration separation is pumped in chromatographic separation device, is with pure water Eluant, with chromatographic isolation resin as separating medium, to nanofiltration membrane separation after final extracting solution in component separate, separate Temperature is 45 DEG C, and separation flow velocity is 1.5m3/ h, extracting solution is separated into two fractions, and a part is based on L-arabinose The content of fraction, wherein L-arabinose is more than 70%;Another part is the fraction based on miscellaneous sugar, collects two kinds respectively and evaporates Point;
The extraction of b, L-arabinose:Take the fraction based on L-arabinose and measure amount of dry matter percent concentration and be 30%, the fraction is concentrated to dryness into amount of substance percent concentration after 50%, to add by the 0.1 of sugar liquid amount of dry matter degree Plus activated carbon, control material temperature is 50 DEG C, and speed of agitator is 60 revs/min, and insulation is filtered after 20 minutes with flame filter press, so By anion-cation exchange resin remove impurity, and it is 65% to be further concentrated to dryness amount of substance percent concentration, imports normal pressure crystallization Crystallization is cooled down in tank, L-arabinose crystal is separated out, most after Jing centrifugations, that drying process obtains L-arabinose is brilliant Body, the purity of L-arabinose crystal is 98.33%, and yield is 86.08%.
Embodiment 3
(1) remove impurity:By 1.0% addition flocculant of sugar liquid amount of dry matter degree in xylose mother liquid, thing is controlled Material temperature degree is 80 DEG C, and speed of agitator is 500 revs/min, is incubated 50 minutes, is then filtered with flame filter press, after obtaining remove impurity Xylose mother liquid;
(2) separating glucose acid sodium:
A, oxydasises:Xylose mother liquid after remove impurity is pumped in immobilized glucose oxidase resin column, temperature 45 C Under constant temperature, oxydasises are carried out, it is 6 times of immobilized glucose oxidase resin volume/hours that xylose mother liquid pumps into speed, until mistake Till flowing out without gluconic acid in the oxydasises liquid of post, oxydasises liquid is collected, carry out ion exchange;
B, anion exchange and regeneration:Oxydasises liquid pump is entered in anion exchange resin, anion exchange is carried out, is pumped into Speed is 6 times of anion exchange resin volume/hours, is monitored by on-line chromatograph work station, until without Fructus Vitis viniferae in effluent Till saccharic acid;In regenerative process, first pump into 3 times of resin anion (R.A.) volume purified water and washed, collect effluent and with before Effluent merges, and by pumping into 8% sodium hydroxide solution eluting is carried out, and the speed that pumps into of sodium hydroxide solution is 4 times of negative resins Volume/hour, without till sodium gluconate in eluent;Eluent is obtained through subsequent concentration, centrifugation, drying steps Gluconic acid sodium crystal, the purity of gluconic acid sodium crystal is 96.13%, and yield is 76.61%;
(3) separating oligomeric xylose:
A, enzymatic conversion are separated with oligomeric xylose:By the pH regulator for removing the xylose mother liquid after glucose to 6, immobilization is pumped into In the fixed bed of xylanase, volume is pumped into for 0.5 times of fixed bed volume/hour, 65 DEG C of fixed bed jacket heat-preservation, from fixed bed Oligomeric xylose content is 12% in the enzymatic conversion liquid of middle outflow, collects the effluent after enzymatic conversion, is directly entered nanofiltration membrane separation System, raffinate is 1 with extracting liquid volume ratio:5, secondary membrance separation is carried out to extracting solution, merge raffinate twice, last raffinate Liquid oligomeric xylose content is 96.99%, and it is 40.01% that extracting solution oligomeric xylose content is 2.34%, Xylose Content, by extracting solution It is by volume 5 with xylose mother liquid after glucose is removed:1 mixing, then Jing enzymatic conversions, membrance separation, until the xylose in extracting solution Content < 10%;
B, extraction oligomeric xylose:Add by the 0.2 of raffinate amount of dry matter degree in nanofiltration membrane separation raffinate Plus activated carbon decolourized, ion exchange remove impurity, be finally concentrated to dryness after amount of substance percent concentration 50% and be spray-dried, Inlet temperature is 180 DEG C, and leaving air temp is 85 DEG C, and charging rate is 1m3/ h, finally obtains xylo-oligosaccharide powder, xylo-oligosaccharide powder Purity be 95.87%, yield is 92.15%;
(4) L-arabinose is separated:
A, L-arabinose are separated:Final extracting solution after by nanofiltration separation is pumped in chromatographic separation device, is with pure water Eluant, with chromatographic isolation resin as separating medium, to nanofiltration membrane separation after final extracting solution in component separate, separate Temperature is 60 DEG C, and separation flow velocity is 3.0m3/ h, extracting solution is separated into two fractions, and a part is based on L-arabinose The content of fraction, wherein L-arabinose is more than 70%;Another part is the fraction based on miscellaneous sugar, collects two kinds respectively and evaporates Point;
The extraction of b, L-arabinose:Take the fraction based on L-arabinose and measure amount of dry matter percent concentration and be 30%, the fraction is concentrated to dryness into amount of substance percent concentration after 70%, to add by the 0.5 of sugar liquid amount of dry matter degree Plus activated carbon, control material temperature is 80 DEG C, and speed of agitator is 150 revs/min, and insulation is filtered after 50 minutes with flame filter press, Then Jing anion-cation exchange resins remove impurity, and it is 75% to be further concentrated to dryness amount of substance percent concentration, imports normal pressure knot Crystallization is cooled down in brilliant tank, make L-arabinose crystal separate out, most after Jing centrifugation, drying process obtain L-arabinose Crystal, the purity of L-arabinose crystal is 99.05%, and yield is 88.78%.

Claims (10)

1. a kind of integrated conduct method of xylose mother liquid, it is characterised in that include:
(1) flocculant, stirring and control material temperature, the xylose mother liquid Jing after filtering and obtain remove impurity are added in xylose mother liquid;
(2) xylose mother liquid after remove impurity is carried out into oxydasises at 35~45 DEG C by immobilized glucose oxidase resin, is obtained Oxidation solution containing gluconic acid, collects oxidation solution and process obtains gluconic acid sodium crystal;
(3) xylose mother liquid for removing glucose is carried out into xylose polyreaction by Immobilized Xylanase bed, is obtained containing low The polymer fluid of xylan, collects polymer fluid and process obtains xylo-oligosaccharide powder;
(4) xylose mother liquid for removing xylose is carried out into chromatographic isolation, the fraction rich in L-arabinose is obtained, at fraction Jing L-arabinose crystal is obtained after reason.
2. the integrated conduct method of xylose mother liquid according to claim 1, it is characterised in that in step (2), controls xylose The speed that mother solution passes through immobilized glucose oxidase resin is 2~6 times of immobilized glucose oxidase resin volume/hours.
3. the integrated conduct method of xylose mother liquid according to claim 1, it is characterised in that in step (2), oxidation solution Process includes:
(2-a) oxidation solution is controlled into the electrical conductivity < 10us/cm of effluent by anion exchange resin;
(2-b) adopt mass percent concentration carries out eluting for 7~10% sodium hydroxide solution to anion exchange resin, washes De- liquid is sodium gluconate solution;Sodium hydroxide solution pumps into anion exchange resin volume/hour that speed is 3~4 times;
(2-c) eluent decolourized, concentrated, being centrifuged, being dried, being obtained gluconic acid sodium crystal.
4. the integrated conduct method of xylose mother liquid according to claim 1, it is characterised in that in step (3), xylose polymerization The pH value of reaction is 5~6, and temperature is 45~65 DEG C, and control removes the xylose mother liquid of glucose and passes through Immobilized Xylanase bed Speed be 0.3~4.5 times of Immobilized Xylanase bed volume/hour.
5. the integrated conduct method of xylose mother liquid according to claim 1, it is characterised in that in step (3), polymer fluid Process includes:
By polymer fluid by the NF membrane that molecular cut off is 100~300KD, volume ratio is obtained for 1:3~5 raffinate with carry Liquid is taken, oligomeric xylose is rich in raffinate, concentrated, centrifugation, drying obtain xylo-oligosaccharide powder.
6. the integrated conduct method of xylose mother liquid according to claim 5, it is characterised in that secondary film is carried out to extracting solution Isolated secondary raffinate and secondary raffinate, raffinate will merge twice.
7. the integrated conduct method of xylose mother liquid according to claim 6, it is characterised in that control merge after raffinate Middle oligomeric xylose content is 90~95%, oligomeric xylose content < 5% in secondary raffinate.
8. the integrated conduct method of xylose mother liquid according to claim 7, it is characterised in that by secondary raffinate with remove The xylose mother liquid of glucose is with volume ratio as 2~5: 1 mixing, aggregated reaction and membrance separation, until in the extracting solution of membrance separation Xylose Content < 10%.
9. the integrated conduct method of xylose mother liquid according to claim 1, it is characterised in that in step (4), be with pure water Eluant, with chromatographic isolation resin as separating medium, the xylose mother liquid to removing glucose and xylose carries out chromatographic isolation, chromatograph point It it is 45~60 DEG C from temperature, eluant flow velocity is 1.5~3.0m3/h。
10. the integrated conduct method of xylose mother liquid according to claim 1, it is characterised in that rich in L-arabinose The process of fraction includes:
(4-a) fraction that will be enriched in L-arabinose is concentrated to dryness amount of substance percent concentration for after 50~70%, dry by sugar liquid 0.1~0.5 addition activated carbon of amount of substance degree, control material temperature is 50~80 DEG C, and speed of agitator is 60~150 Rev/min, insulation is filtered after 20~50 minutes;
(4-b) by filtrate Jing ion exchange resin remove impurity, and it is 65~75% to be further concentrated to dryness amount of substance percent concentration, Jing cooling crystallizations, centrifugation, drying, obtain L-arabinose crystal.
CN201611194776.7A 2016-12-21 2016-12-21 Comprehensive treatment method of xylose mother liquor Pending CN106591384A (en)

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